反应详情

温度

0 °C

5 g 4-(Methylamino)butan-1-ol (0.049 mol) is slowly added to 15 g HNO3 (100%, 0.24 mol) at −10° C., care being taken that the temperature does not rise above 10° C. The mixture is stirred for 10 min at 0° C., then poured on ice (15 g) and stirred for 2 h at room temperature. 33 g 2-Butanol is added slowly at 0° C., the obtained mixture (pH 0-1) neutralised (to pH 6) with 15.6 g NaHCO3 at 0° C., filtered and the organic phase dried over MgSO4. 1.2 g Norrit 2× is added, the mixture filtered, and the filtrate evaporated to give 5.4 g (52%) N-methyl-N-(4-nitroxybutyl)ammonium nitrate. 1H-NMR (200 MHz, DMSO-d6): 1.56-1.78 (m, 4H); 2.54 (t, J=5.5, 3H); 2.84-2.97 (m, 2H); 4.52 (t, J=5.9, 2H); 8.30 (br. s, 2H).

1. customdoes not rise above 10° C
2. additionpoured on ice (15 g)
3. stirringstirred for 2 h at room temperature
4. customat 0° C.
5. filtrationfiltered
6. dry with materialthe organic phase dried over MgSO4
7. addition1.2 g Norrit 2× is added
8. filtrationthe mixture filtered
9. customthe filtrate evaporated